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S.C. acknowledges the FCT grant, ref. 2021.08212.BD. F.J.F-.A. acknowledges the Formacion de Profesorado Universitario programme, ref. FPU22/04365. S.M.G. acknowledges the FCT grant, ref. 2024.01570.BD. IST authors acknowledge FCT (Portugal) support through contracts UIDB/04349/2020 and the National Infrastructure Roadmap, LTHMFL-NECL, LISBOA-01-0145-FEDER-022096. A.A. acknowledges FCT-Fundacao para a Ciencia e a Tecnologia for her contract DL57/2016 (ref. DL 57/2016/CP1454/CT0017) with DOI: 10.54499/DL57/2016/CP1454/CT0017 (10.54499/DL57/2016/CP1454/CT0017) and Projects H2FlexiPEC's (ref. 2022.07332.PTDC) with DOI: 10.54499/2022.07332.PTDC (10.54499/2022.07332.PTDC); IFIMUP-UIDB/04968/2020 (DOI: 10.54499/UIDB/04968/2020), UIDB/04968/2021 (DOI: 10.54499/UIDB/04968/2021), LapMET-LA/P/0095/2020 DOI (10.54499/LA/P/0095/2020); 2024.00223.CERN; COST Action NETPORE (CA20126)/OC-2020-1-24842. C.T.d.S. acknowledges the program Atraccion de Talento (Comunidad Autonoma de Madrid), ref. 2020-T1/IND-19889, and Agencia Estatal de Investigacion for the project PID2022-141080OB-C22.

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Anisotropic Porous Iron-Based Nanoparticles through Two-Step Hydrothermal and Hydrogen-Based Reduction: Enhanced Magnetic Performance for Potential Biomedical Applications

Publicado en:Acs Applied Materials & Interfaces. 17 (11): 16602-16615 - 2025-03-07 17(11), DOI: 10.1021/acsami.4c21063

Autores: Caspani S; Fernández-Alonso FJ; Gonçalves SM; Martín-Morales C; Cortes-Llanos B; Vieira BJC; Waerenborgh JCB; Pereira LCJ; Apolinario A; Araújo JP; Gómez-Gaviro MV; Torres-Costa V; Manso Silván MJ; de Sousa CT

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Iron-based nanoparticles have emerged as promising candidates for diverse biomedical applications, including cell separation, targeted drug delivery, hyperthermia therapy, and magnetic resonance imaging. This study reports the scalable synthesis of high-magnetization iron-based nanoparticles with controlled anisotropic shapes, achieved via a two-step process. Hematite nanoparticles, featuring nanocube, nanoellipse, and nanoneedle morphologies, were synthesized through the hydrolysis of ferric chloride in the presence of ammonium dihydrogen phosphate, with the morphology precisely tuned by adjusting reagent concentrations. These hematite nanoparticles were subsequently reduced in a hydrogen-based direct reduction at 480 degrees C, yielding iron-magnetite nanocomposites that retained their anisotropic shapes, exhibited significant porosity, and achieved an exceptional saturation magnetization of 207 emu/g - approximately 150% higher than conventional magnetite nanoparticles. Comprehensive characterization via SQUID magnetometry, Mossbauer spectroscopy, Rietveld refinement of X-ray diffraction data, and XPS for surface analysis confirmed the formation of metallic iron nanoparticles covered by a magnetite shell. Biocompatibility studies demonstrated the biocompatibility of these nanoparticles across a wide concentration range, underscoring their suitability for biomedical applications.

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